3,4-环氧环己基甲酸-3′,4′-环氧环己基甲酯的制备  

Preparation of 3,4-epoxycyclohexylmethyl-3′,4′–epoxy-cyclohexane carboxylate

作　　者：冯韶静 宋玉婉 熊健西 肖亚平[1] Feng Shaojing;Song Yuwan;Xiong Jianxi;Xiao Yaping(School of Chemistry and Materials Science,Nanjing Normal University,Nanjing 210023,China)

机构地区：[1]南京师范大学化学与材料科学学院,江苏省南京市210023

出　　处：《合成树脂及塑料》2018年第6期10-14,共5页China Synthetic Resin and Plastics

摘　　要：在无催化剂、室温条件下由3-环己烯甲酸-3′-环己烯甲酯(简称A)环氧化反应合成3,4-环氧环己基甲酸-3′,4′-环氧环己基甲酯(AOO)。以环境友好的H_2O_2为氧源,1,2-二氯乙烷为溶剂,考察了n(A)∶n(H_2O_2)、反应温度、反应时间、溶剂用量、除水剂用量、缓冲剂用量等对反应的影响。结果表明,以25 mmol的A计,适宜的合成条件,1,2-二氯乙烷16 mL,n(A)∶n(H_2O_2)为1.0∶3.5,A与乙酸酐摩尔比为1∶4,A与无水乙酸钠摩尔比为1.0∶0.5,室温条件下反应2.5 h。在该条件下,经气相监测得A的转化率达99.0%,AOO的产率达90%以上,纯度达99.03%。3,4-epoxycyclohexylmethyl-3′,4′-epoxycyclohexane carboxylate(AOO)was synthesized via the epoxidation of 3-cyclohexenylmethyl-3′-cyclohexene carboxylate(A)under the conditions of catalyst free and room temperature.Environmentally-friendly hydrogen peroxide was used as oxygen source and 1,2-dichloroethane as solvent to observe the effects of the molar ratio of A and H2O2,reaction temperature,reaction time,amount of solvent,dehydrating agent and buffer on the reaction.The results show that the optimal synthetic conditions in the presence of A of 25 mmol are as follows:A of 25 mmol,1,2-dichloroethane of 16 mL,the molar ratio of A/H2O2,A/acetic anhydride and A/anhydrous sodium acetate are 1.0∶3.5,1∶4,1.0∶0.5 respectively,and reacted at room temperature for 2.5 h.The test results from gas phase monitoring indicate that under these conditions the conversion rate of A is up to 99%,the yield of AOO is beyond 90%,and the purity of the product reaches 99.03%.

关 键 词：3-环己烯甲酸-3′-环己烯甲酯 3 4-环氧环己基甲酸-3′ 4′-环氧环己基甲酯 环氧化反应 过氧化氢 

分 类 号：TQ323.5[化学工程—合成树脂塑料工业]